반응 #64946

ord-f0e21d3541234709a7e0200795083ab8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITAfter the mixture has been left
  2. 2
    기타On purification by chromatography, impurities
  3. 3
    세척are first eluted with ethyl acetate
  4. 4
    세척the product is then eluted with ethyl acetate:methanol (3:1) (RF value 0.55)

실험 절차

17.4 g (0.58 mmol ) of sodium hydride suspension are reacted with 119 g (0.45 mol) of 1-benzyl-3-(2-chloroethylamino)-pyrrolidine-2,5-dione in 550 ml of absolute dimethylformamide in accordance with the working instructions of Example Ib. After the mixture has been left to stand overnight, it is worked up under aqueous conditions. On purification by chromatography, impurities are first eluted with ethyl acetate and the product is then eluted with ethyl acetate:methanol (3:1) (RF value 0.55). 57.7 g of product (56% of theory) are isolated.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05416096uspto-grants-1995_05